CN103930250A - Preparation of inorganic samples by fusion - Google Patents
Preparation of inorganic samples by fusion Download PDFInfo
- Publication number
- CN103930250A CN103930250A CN201280051961.4A CN201280051961A CN103930250A CN 103930250 A CN103930250 A CN 103930250A CN 201280051961 A CN201280051961 A CN 201280051961A CN 103930250 A CN103930250 A CN 103930250A
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- CN
- China
- Prior art keywords
- mould
- crucible
- mixture
- methods according
- inert gas
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
- B22D21/02—Casting exceedingly oxidisable non-ferrous metals, e.g. in inert atmosphere
- B22D21/025—Casting heavy metals with high melting point, i.e. 1000 - 1600 degrees C, e.g. Co 1490 degrees C, Ni 1450 degrees C, Mn 1240 degrees C, Cu 1083 degrees C
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D25/00—Special casting characterised by the nature of the product
- B22D25/02—Special casting characterised by the nature of the product by its peculiarity of shape; of works of art
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
In a process for the preparation of inorganic sample disks for analysis, the sample, in powdered form, is mixed with a powdered reagent flux which has been pre-melted. In an inert gas atmosphere, the mixture is placed in a graphite crucible and heated to a temperature slightly above 1000 DEG C. After the flux dissolves the sample, a homogenous mix is produced. This mix is then poured into a graphite mold, the bottom of which contains a molten pool of an inert metal, such as gold, which acts as a smooth receiving surface. Upon cooling, the material in the mold solidifies, resulting in a glassy disk that can be analyzed. Cooling can be accelerated by making use of a cooling fluid that has a substantially higher thermal capacity than air.
Description
Technical field
The present invention relates generally to the preparation of the inorganic samples of being undertaken by fusion, and relates more specifically to prepare by fusion the improved method and system of inorganic samples.
Background technology
In the known existing preparation technology for the inorganic samples analyzed, will there is the sample (geological, mineralogical or some inorganic material) and the Powdered reagent mix that is called as flux of powdery form.Mixture is placed in platinum-billon crucible, and is heated to the temperature a little more than 1000 DEG C.At this temperature, flux will melt within a few minutes, and the oxide existing in sample dissolution, and then produce uniform mixture.Afterwards, the mixture of this fusing is filled in the mould of being made up of the alloy identical with crucible.After cooling, the material in mould will solidify, and then generate analyzable glassy dish.
This technique at least shows following defect:
In some cases, this process is by the time very long cost;
Crucible and mould cause their cost very high owing to being made up of precious metal;
For some sample, molten material is thickness very, and makes glassy dish damaged;
Melt viscosity also can cause the deteriorated fast of mould;
The surface of mould must be completely smooth and smooth as much as possible, otherwise will there will be analytical error;
Need again polishing die surface to keep this slickness;
Owing to can not preparing with the risk of crucible fusion the sample that comprises platinum or gold (or other precious metals).
Summary of the invention
In a broad sense, the object of the present invention is to provide the method and system for the preparation of inorganic samples, the method and system have overcome existing methodical more than one defect.Special expectation, the method and system are easy to use and use is reliable, and advantageously should realize compared with the conventional method cost savings.
According to an aspect of the present invention, guarantee the smooth receiving surface for mixture, and by pouring into uniform mixture on the surface, inertia deposite metal such as liquid gold, made again the workload of polished surface minimize.
According to a further aspect in the invention, by fritting flux in heating clamber and by itself and the speed that improves the method in the sample mix of liquid condition.Also desirably, be generally used for cooling and have substantially higher than the liquid of the thermal capacitance of air and carry out cooled glass shape dish by use, thereby improving the speed of the method.Preferred liquid comprises water and liquid gas, and wherein these liquid gas are very ice-cold in the time that the storage form from them is depressurized as atmospheric pressure.
According to a further aspect in the invention, by do not use by precious metal (such as, platinum-billon, below also referred to as " platinum appliance ") crucible made, and replace the crucible of being made by glassy graphite (below also referred to as " graphite vessel "), can realize cost savings.But because graphite in the time that oxygen exists is at high temperature deteriorated rapidly, therefore, this process must be carried out in inert gas environment, preferably carries out in the gaseous environment that contains nitrogen, argon gas or neon or its combination.
Brief description of the drawings
With reference to accompanying drawing, can be according to of the present invention preferably current but only for exemplary embodiment is come comprehend aforementioned brief description of the present invention and other objects, features and advantages.Wherein, as being the schematic diagram for prepare the system of inorganic samples by fusion for the Fig. 1 that embodies unique accompanying drawing of the present invention.
Detailed description of the invention
Comprise and heating comprising through the crucible of the lithium borate flux of fine gtinding and the mixture of sample itself according to the preparation of inorganic samples of being undertaken by fusion of the present invention.Conventionally the lab assistant of, carrying out this process also will add halogen compounds to remove final products to facilitate.Lithium borate sample dissolution, and can promote this dissolving by stirring crucible.After complete reaction, the hot solution obtaining is filled in tabular mould, and it is cooling, to generate the glassy dish that can use easily subsequently in elemental analyser.
Fig. 1 is of the present invention for prepare the schematic diagram of system 10 of inorganic samples by fusion.All processes are carried out in main shell 12, and wherein main shell 12 is preferably bubble-tight.Continue shell 12 to fill the inert gas such as nitrogen, argon gas or neon from below, even if select above-mentioned gas also can suppress oxidation reaction and other reactions at the temperature very high.The main application of this gas is to avoid the oxidation of the assembly such as such as crucible 14 and mould 16 of enclosure, and this will be further discussed hereinafter.
Fresh inert gas is transported to input sash 18 for sample being added to main shell 12 and in the output sash 20 that the sample after completing is fetched from main shell 12.In order to make the minimization of loss of gas, input sash 18 and output sash 20 are designed with the door that allows gas flow to enter main shell 12 but can not flow out from main shell 12.Can any excess air being gathered in main shell 12 be discharged via the exhaust apparatus 22 at main shell 12 tops, preferably be expelled to existing laboratory hood pipe-line system (not shown).
Sample is fed in main shell 12 by input sash 18, and is retained in the crucible 14 of being made up of graphite.Because the crucible using in this type of technique is made up of very expensive platinum-billon conventionally, therefore use graphite crucible to realize sizable saving.The use of inert gas environment has been avoided causing crucible in inner occur deteriorated of main shell 12 because the temperature in technique exceedes 1000 DEG C in the situation that there is oxygen, thereby makes graphite crucible become effective substitute.Crucible 14 use heaters 24 heat, and be positioned at directly over mechanical support 26, and mechanical support 26 is positioned on electronic scale (and system controller) 28 to ensure thermometric stability, and wherein electronic scale (and system controller) 28 is positioned at the outside of shell 12.Weighing apparatus 28 detects the quality of sample, and system controller calculates the quality of the flux that will add.
Powdered flux 30 is stored in the funnel 33 of shell 12 tops.Flux is fused into liquid state by the heater 31 that is arranged in funnel 33 bottoms.Regulate the interpolation of flux to crucible 14 by the servo valve 35 of being controlled by controller 28.Therefore, can be to the flux that adds accurate dosage in the sample in crucible.The heat being provided by heater 24 in existence, sample is dissolved in flux.By inject flux instead of the conventional Powdered flux of existing technique of fusing to crucible, can accelerate the dissolving of sample.
Once sample is dissolved completely, as indicated in the arrow pointing to downwards from Powdered flux 30, by inclination crucible 14, sample is filled in mould 16.
Die assembly 16 comprises the rigid container for holding the material that can again melt 32 such as gold.Compared with the flux of this material and fusing, should have larger density, with respect to material should be inertia, its fusing point should and should not adhere to flux lower than 1200 DEG C.In the time that sample is also in crucible, make gold fusing, form thus smooth receiving surface.After perfusion, flux swims in the gold top of fusing.Afterwards, below mould 16, inject inert gas by operated valve 34 with cooling die 16, thereby form glassy dish at golden top.The bottom of mould 16 is smooth, polished surface, but inwall is coning emptied on its top, easily to remove dish.
The bottom of mould 16 comprises undercutting slot part 36 so that gold is kept in mould.That is, in the time removing glassy dish, due to the curing gold forming towards crucible bottom as shown in the figure, curing gold can be kept to the appropriate location of crucible bottom, this keeps gold in position, and only allows glassy dish to remove.
The sample of dissolving is filled on the receiving surface of inertia deposite metal, can guarantees that sample is always in smoothly and not needing constantly again on polished surface.
In order to accelerate this process, can expect, carry out cooling die by introducing the liquid substantially with higher thermal capacitance, instead of carry out cooling die with inert gas.Preferred liquid comprises water and liquid gas, and wherein these liquid gas are very ice-cold the process that is depressurized into atmospheric pressure from their file layout.
Although disclose for illustrative purposes the preferred embodiments of the present invention, technical staff multiplely supplements understanding in the case of not deviating from by realizing the clear and definite scope and spirit of the present invention of the claim of enclosing, amendment and replacing.
Claims (29)
1. for carry out a method for perparation of specimen dish by Powdered inorganic samples, it comprises the steps:
In crucible by Powdered reagent and described sample mix;
Heat described crucible to obtain the mixture that is dissolved with described sample;
Described mixture is filled in mould, described mould comprises the deposite metal as the reception basal surface for described mixture, described deposite metal have compared with described mixture larger density, with respect to described mixture be substantially inertia, do not adhere to described mixture and there is the fusing point lower than 1200 DEG C; And
Cooling described mixture in described mould, so that formation dish.
2. method according to claim 1, wherein, carries out the mould that described method uses and has interior diapire and near the inward flange being formed by undercutting described diapire, makes the inside of described mould near described diapire, have cumulative lateral dimension.
3. method according to claim 1, wherein, described metal is gold or golden alloy.
4. method according to claim 3 wherein, melted described reagent before described blend step.
5. method according to claim 4, wherein, described cooling step comprises introduces the liquid having substantially higher than the thermal capacitance of air.
6. method according to claim 5, wherein, described liquid is water or the liquefaction that is depressurized after introducing.
7. method according to claim 5, wherein, described crucible and described mould are made up of graphite, and described method is carried out in the environment being substantially made up of inert gas.
8. method according to claim 7, wherein, described inertia is the member in rare gas group.
9. method according to claim 1 wherein, melted described reagent before blend step.
10. method according to claim 1, wherein, described cooling step comprises introduces the liquid having substantially higher than the thermal capacitance of air.
11. methods according to claim 1, wherein, described crucible and described mould are made up of graphite, and described method is carried out in the environment being substantially made up of inert gas.
12. methods according to claim 11, wherein, described inert gas comprises the member in the group of containing nitrogen, argon gas and neon.
13. 1 kinds for carrying out the method for perparation of specimen dish by Powdered inorganic samples, it comprises the steps:
In crucible by fusing Powdered reagent and described sample mix;
Heat described crucible to obtain the mixture that is dissolved with described sample;
Described mixture is filled in mould; And
In described mould, cooling described mixture coils with formation.
14. methods according to claim 13, wherein, described cooling step comprises introduces the liquid having substantially higher than the thermal capacitance of air.
15. methods according to claim 14, wherein, described liquid is water or the liquefaction that is depressurized after introducing.
16. methods according to claim 14, wherein, described crucible and described mould are made up of graphite, and described method is carried out in the environment being substantially made up of inert gas.
17. methods according to claim 16, wherein, described inert gas comprises the member in the group of containing nitrogen, argon gas and neon.
18. methods according to claim 13, wherein, described cooling step comprises introduces the liquid having substantially higher than the thermal capacitance of air.
19. methods according to claim 13, wherein, described crucible and described mould are made up of graphite, and described method is carried out in the environment being substantially made up of inert gas.
20. methods according to claim 19, wherein, described inert gas comprises the member in the group of containing nitrogen, argon gas and neon.
21. 1 kinds for carrying out the method for perparation of specimen dish by Powdered inorganic samples, it comprises the steps:
In crucible by Powdered reagent and described sample mix;
Heat described crucible to obtain the mixture that is dissolved with described sample;
Described mixture is filled in mould; And
There is substantially the liquid higher than the thermal capacitance of air, cooling described mixture in mould, thereby formation dish by introducing.
22. methods according to claim 21, wherein, described liquid is water or the liquid gas that is depressurized after introducing.
23. methods according to claim 21 wherein, melted described reagent before described blend step.
24. methods according to claim 21, wherein, described crucible and described mould are made up of graphite, and described method is carried out in the environment being substantially made up of inert gas.
25. methods according to claim 24, wherein, described inert gas comprises the member in the group of containing nitrogen, argon gas and neon.
26. 1 kinds for carrying out the method for perparation of specimen dish by Powdered inorganic samples, it comprises the steps:
In the crucible of being made by graphite by Powdered reagent and described sample mix;
Heat described crucible to obtain the mixture that is dissolved with described sample;
Described mixture is filled in the mould of being made by graphite; And
In described mould, cooling described mixture to be to form described dish,
Described method is carried out in the environment being substantially made up of inert gas, and the bottom of described mould is coated with metal.
27. methods according to claim 26, wherein, described inert gas comprises the member in the group of containing nitrogen, argon gas and neon.
28. methods according to claim 26 wherein, melted described reagent before described blend step.
29. methods according to claim 26, wherein, described cooling step comprises introduces the liquid having substantially higher than the thermal capacitance of air.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US13/220,904 | 2011-08-30 | ||
| US13/220,904 US8403025B2 (en) | 2011-08-30 | 2011-08-30 | Preparation of inorganic samples by fusion |
| PCT/US2012/052783 WO2013033153A1 (en) | 2011-08-30 | 2012-08-29 | Preparation of inorganic samples by fusion |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103930250A true CN103930250A (en) | 2014-07-16 |
| CN103930250B CN103930250B (en) | 2016-10-19 |
Family
ID=47742501
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201280051961.4A Expired - Fee Related CN103930250B (en) | 2011-08-30 | 2012-08-29 | Inorganic samples is prepared by fusion |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US8403025B2 (en) |
| EP (1) | EP2750849B1 (en) |
| KR (1) | KR20140091518A (en) |
| CN (1) | CN103930250B (en) |
| AU (1) | AU2012302126B2 (en) |
| ES (1) | ES2725789T3 (en) |
| WO (1) | WO2013033153A1 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160003720A1 (en) * | 2014-07-07 | 2016-01-07 | Spex Sample Prep Llc | Apparatus Comprising an Increased-Capacity Platinumware Holder and Method Therefor |
| WO2016041063A1 (en) * | 2014-09-15 | 2016-03-24 | Materiaux Nieka Inc. | Method and apparatus for preparing an analytical sample by fusion |
| CN104197008A (en) * | 2014-09-28 | 2014-12-10 | 无锡市新颖密封材料厂 | Production technology for graphite gasket |
| US10814388B2 (en) | 2018-01-24 | 2020-10-27 | General Electric Company | Heated gas circulation system for an additive manufacturing machine |
| US10814395B2 (en) | 2018-01-24 | 2020-10-27 | General Electric Company | Heated gas circulation system for an additive manufacturing machine |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1357003A (en) * | 1971-02-04 | 1974-06-19 | British Aircraft Corp Ltd | Production of foamed synthetic resin materials |
| US4865784A (en) * | 1989-02-21 | 1989-09-12 | Hill Francis U | Method of making porous inorganic particle filled polyimide foam insulation products |
| CN101454138A (en) * | 2005-12-16 | 2009-06-10 | 诚盟塑胶制品（东莞）有限公司 | Method and device for manufacturing plastic product |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2381303A1 (en) * | 1977-02-21 | 1978-09-15 | Siderurgie Fse Inst Rech | APPARATUS FOR THE AUTOMATIC PREPARATION OF SAMPLES INTENDED FOR X-FLUORESCENCE ANALYSIS |
| JPS6027847A (en) * | 1983-07-26 | 1985-02-12 | Nippon Steel Corp | Preparation of specimen for fluorescent x-ray analysis |
| FR2556095B1 (en) * | 1983-12-02 | 1986-09-05 | Philips Ind Commerciale | AUTOMATIC SAMPLE DOSING PROCESS AND AUTOMATIC MACHINE FOR DOSING AND ANALYZING |
| US5269827A (en) * | 1991-03-01 | 1993-12-14 | Leco Corporation | Analytical sample preparation system |
| JPH1164186A (en) * | 1997-08-18 | 1999-03-05 | Daido Steel Co Ltd | Preparing method for specimen for fluorescent x-ray analysis |
| DE10361525B4 (en) * | 2003-12-23 | 2005-11-17 | Umicore Ag & Co. Kg | Process for the preparation of orodispersible tablets for the determination of the content of ceramic powders on platinum group metals by means of RFA |
| AU2007202703B2 (en) * | 2007-05-04 | 2009-01-15 | X-Ray Flux Pty Ltd | X-ray flux composition |
| AU2010249195B1 (en) * | 2010-12-07 | 2011-06-30 | X-Ray Flux Pty Ltd | Lithium X-Ray flux composition |
-
2011
- 2011-08-30 US US13/220,904 patent/US8403025B2/en active Active
-
2012
- 2012-08-29 KR KR1020147008556A patent/KR20140091518A/en not_active Application Discontinuation
- 2012-08-29 WO PCT/US2012/052783 patent/WO2013033153A1/en active Application Filing
- 2012-08-29 AU AU2012302126A patent/AU2012302126B2/en not_active Ceased
- 2012-08-29 ES ES12828170T patent/ES2725789T3/en active Active
- 2012-08-29 CN CN201280051961.4A patent/CN103930250B/en not_active Expired - Fee Related
- 2012-08-29 EP EP12828170.6A patent/EP2750849B1/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1357003A (en) * | 1971-02-04 | 1974-06-19 | British Aircraft Corp Ltd | Production of foamed synthetic resin materials |
| US4865784A (en) * | 1989-02-21 | 1989-09-12 | Hill Francis U | Method of making porous inorganic particle filled polyimide foam insulation products |
| CN101454138A (en) * | 2005-12-16 | 2009-06-10 | 诚盟塑胶制品（东莞）有限公司 | Method and device for manufacturing plastic product |
Also Published As
| Publication number | Publication date |
|---|---|
| EP2750849A4 (en) | 2015-08-26 |
| EP2750849A1 (en) | 2014-07-09 |
| EP2750849B1 (en) | 2019-02-20 |
| ES2725789T3 (en) | 2019-09-27 |
| US8403025B2 (en) | 2013-03-26 |
| WO2013033153A1 (en) | 2013-03-07 |
| KR20140091518A (en) | 2014-07-21 |
| AU2012302126B2 (en) | 2017-01-12 |
| CN103930250B (en) | 2016-10-19 |
| AU2012302126A1 (en) | 2014-04-17 |
| US20130049247A1 (en) | 2013-02-28 |
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| C14 | Grant of patent or utility model | ||
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Granted publication date: 20161019 Termination date: 20170829 |